CN111795764B - Sandwich type large-area high-density flexible array sensor and preparation method thereof - Google Patents
Sandwich type large-area high-density flexible array sensor and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the field of sensors, and discloses a sandwich type large-area high-density flexible array sensor and a preparation method thereof, wherein the sensor comprises an upper polar plate, a lower polar plate, an array pressure-sensitive layer and an insulating adhesive layer, wherein the array pressure-sensitive layer and the insulating adhesive layer are arranged between the upper polar plate and the lower polar plate, the upper polar plate and the lower polar plate are provided with corresponding array electrodes and leads, the array electrodes are in a row-column line structure, each column of electrodes are connected through the leads, and the position of the insulating adhesive layer, which corresponds to the array pressure-sensitive layer, is hollowed out, and the preparation method comprises the following steps: preparing an upper polar plate and a lower polar plate by adopting a screen printing process; preparing a pressure-sensitive composite material; printing an uncured pressure-sensitive composite material on the array electrode on one of the polar plates by adopting a screen printing process to form an array pressure-sensitive layer; and (4) attaching the upper and lower polar plates through insulating glue. The method has the advantages of simple process, higher efficiency and low cost, and the prepared large-area high-density flexible array sensor has high sensitivity, good stability and large pressure sensing range.
Description
Technical Field
The invention relates to the field of sensors, in particular to a sandwich type large-area high-density flexible array sensor and a preparation method thereof.
Background
With the improvement of scientific technology and modernization level, the requirement of people on pressure monitoring is higher and higher, the pressure monitoring on a regular rigid surface is not limited any more, the modes are also various, and the common rigid sensor can not meet the actual requirements of people. The flexible pressure sensor can be bent or even folded at will, is small in size and thin in thickness, and the flexible material is basically non-toxic and harmless, so that the flexible pressure sensor has good compatibility with a human body, and is widely researched and applied in the fields of medical equipment, intelligent robot bionic skin, wearable equipment and the like in recent years.
In recent years, with rapid development in the fields of robot bionic skin, flexible wearable equipment and the like, people have increasingly raised requirements on large-area high-density flexible sensor arrays, and although flexible pressure sensor technology has been developed greatly in recent years, research on large-area flexible array sensors is less.
In large area integration applications, a soft lithography process is generally adopted at present, for example, in chinese patent document, "a flexible wearable resistive strain sensor and a method for making the same", which is disclosed in publication No. CN108267078A, the resistive strain sensor includes a flexible substrate, a sensing layer, an electrode layer, and a protective layer. Compared with other sensors of the same type, the sensor has the characteristics of rapid large-area preparation, good stability, high sensitivity, simple and convenient operation and the like.
However, the sensor adopting the traditional photoetching process has low material utilization rate and overhigh manufacturing cost, and when the sensor is integrated in a large area, if the array density is higher, the efficiency is too low, the preparation difficulty is overlarge, and the application of the sensor is limited.
Disclosure of Invention
The invention provides a sandwich type large-area high-density flexible array sensor and a preparation method thereof, aiming at overcoming the problems that the traditional photoetching process is adopted to prepare the large-area flexible sensor in the prior art, the material utilization rate is low, the manufacturing cost is overhigh, and the efficiency is too low and the preparation difficulty is overlarge if the array density is higher during large-area integration.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a sandwich type large-area high-density flexible array sensor comprises the following steps:
(1) preparing a polar plate: respectively printing electrode materials on the two substrate materials by adopting a screen printing process, forming an array electrode and a lead which correspond to each other on the two substrate materials, and drying to obtain an upper polar plate and a lower polar plate;
(2) preparing a pressure-sensitive composite material: the conductive particles and 5-20 parts of nano SiO by weight2And 15-40 parts of silane coupling agent Si-69 are dispersed in 85-115 parts of solvent to form dispersion liquid; adding 350-450 parts of silicon rubber into the dispersion liquid, and uniformly stirring to obtain a mixed liquid; vacuum drying the mixed solution for 20-30min to obtain an uncured pressure-sensitive composite material, wherein the conductive particles comprise 20-75 parts of carbon black and 5-25 parts of carbon nanotubes;
(3) manufacturing a pressure-sensitive layer of the sensor array: printing an uncured pressure-sensitive composite material on the array electrode on one of the polar plates by adopting a screen printing process, and forming an array pressure-sensitive layer after curing;
(4) packaging a sensor: and (4) attaching the upper and lower polar plates through insulating glue.
The polar plate and the array pressure-sensitive layer are manufactured by adopting a screen printing process, so that the process can be simplified, the cost can be reduced, and the processing efficiency can be improved. The silicon rubber is selected as a matrix material in the pressure-sensitive composite material, and has excellent electrical insulation performance and aging resistance, high mechanical strength, good elasticity, ultraviolet light resistance, ozone resistance, acid and alkali resistance, wide use temperature range, safety, no toxicity, good compatibility with a human body and excellent processability; the silicon rubber is doped with conductive particles, so that the silicon rubber has certain conductivity and certain pressure-sensitive performance.
The pressure-sensitive composite material of the invention adopts carbon black and carbon nano tubes as conductive particles, and the carbon black/carbon nano tubes can play a role of synergistic enhancement when being used together in the silicone rubber due to the larger length-diameter ratio of the carbon nano tubes and the relatively shorter silicone rubber molecular chains. The carbon black and the carbon nano tube can form a structure similar to a grape string, the carbon nano tube can be regarded as a stem and has the function of linking and fixing the carbon black, and the silicon rubber molecular chain is used as a framework of a conductive network chain and is mutually staggered with the grape string-shaped structure to form a stable reinforcing structure. Due to the larger length-diameter ratio of the carbon nano tube, the carbon nano tube can play a role in long-distance electric conduction in a system, and the carbon black can play a role in short-distance electric conduction on one hand and can also connect adjacent carbon nano tubes to play a role in bridging. The integral reinforcing structure has certain influence on the conductivity and stability of the composite system and the mechanical property of the composite material. Compared with a single system, the mechanical property is improved, the conductive network with the dotted line structure has higher sensing sensitivity, the number of conductive channels is increased in a certain pressure range, and the pressure sensing range is improved, so that the sensitivity and the measuring range of the sensor are improved.
The proportion of each component of the pressure-sensitive composite material is suitable for a screen printing process, the composite material can well penetrate through a screen printing plate during printing, the performance after printing is good, the film thickness is uniform and smooth, and the phenomena of paste surface deformation and the like are avoided.
Since the electrode, the lead and the pressure-sensitive layer prepared in the invention are directly printed on the substrate material, the sensor is easy to fall off or scratch to cause damage during the use process, the measured data is inaccurate if the measured data is light, and the sensor fails if the measured data is heavy. And the electrode material is exposed to air for a long time, so that oxidation reaction is easy to occur, the conductivity of the lead is deteriorated, and the performance of the sensor is seriously influenced. Therefore, the upper and lower polar plates are attached by the insulating adhesive layer, so that the contact between the electrode and the wire and the air can be isolated, and the pressure-sensitive layer can be protected from being damaged.
Preferably, the electrode material in step (1) is a yutelin type ID01 conductive silver paste, and the base material is a PET substrate. The conductive silver paste has good conductivity and good fluidity, is suitable for screen printing, and the prepared electrode and lead have good strength and pressure resistance and strong adhesive force on a substrate material.
Preferably, a 300-420-mesh steel wire mesh plate or a polyester mesh plate is adopted during screen printing in the step (1), the electrode material can well penetrate through the screen plate during printing, and the printed electrode and the printed lead are uniform and smooth and have good performance.
Preferably, the drying temperature in the step (1) is 120-140 ℃, and the drying time is 40-60 min. The printed electrode and the printed lead can be better cured and formed and attached to the surface of the base material, so that the prepared upper and lower polar plates have good performance.
Preferably, the conductive particles in step (2) are surface-modified conductive particles, and the preparation method thereof is as follows:
(A) dispersing conductive particles in 0.4-0.6mol/L nitric acid solution, carrying out oscillation reaction for 2-3h, filtering, washing with water to neutrality, and drying at 60-70 ℃ for 12-24 h;
(B) dissolving the obtained product in thionyl chloride, adding 2-3 drops of N, N-dimethylformamide, and reacting at 50-60 ℃ for 12-24 h; (C) dispersing the obtained product in ethylene glycol, and carrying out reflux reaction at the temperature of 100-120 ℃ for 20-30 h;
(D) mixing 4-dimethylamino pyridine and triethylamine in the mass ratio of 1 (10-15) to (15-20) and the product obtained in the step (C), adding CHCl3Adding a chloroform solution of 2-bromoisobutyl acyl bromide with the mass ratio of 1:1-2:1 to the product obtained in the step (C) under the protection of nitrogen, stirring at 0-4 ℃ for 1-2h, and continuing to react at room temperature for 20-30 h;
(E) diluting the obtained solution with chloroform, filtering, repeatedly washing, and drying at 50-60 deg.C for 10-20 h;
(F) mixing the dried pentamethyl diethylenetriamine and CuBr in the mass ratio of 1 (1-2) to 5-7 with the product obtained in the step (E), adding N, N-dimethylformamide, adding vinyl pyrrolidone in the mass ratio of 10:1-15:1 with the product obtained in the step (E) under the protection of nitrogen, and stirring and reacting for 20-30h at the temperature of 60-70 ℃;
(G) and after the obtained solution is filtered, washing the solution to be neutral by water, and drying the solution for 6 to 12 hours at the temperature of between 60 and 70 ℃ to obtain the surface modified conductive particles.
Introducing carboxylic acid groups on the surfaces of the conductive particles through nitric acid treatment; then reacting with thionyl chloride in the step (B) to obtain conductive particles for acyl chlorination; then, conducting reaction with ethylene glycol in the step (C) to obtain surface hydroxylated conductive particles; reacting with a brominating reagent in the step (D) to obtain brominating conductive particles; and (F) initiating vinyl pyrrolidone monomer polymerization by using the brominated conductive particles as an initiator, and grafting the vinyl pyrrolidone monomer on the surface of the conductive particles to finally obtain the surface modified conductive particles.
Because carbon black and carbon nano tubes both have larger specific surface area and surface energy, larger interparticle force is easy to be wound and agglomerated with rubber, so that the dispersibility of the carbon black and the carbon nano tubes is poor, and the performance of the pressure-sensitive composite material is influenced. According to the invention, the dispersant polyvinylpyrrolidone is grafted on the surface of the conductive particle, so that the hydrophobic group of the dispersant is firmly adsorbed on the surface of the conductive particle, the hydrophilic group extends in an aqueous system, the surface free energy of the conductive particle is reduced, the steric hindrance is increased, and the conductive particle after surface modification has high dispersion stability, thereby improving the piezoresistive performance of the pressure-sensitive composite material and improving the sensitivity of the sensor.
Preferably, the solvent in step (2) comprises at least one of n-hexane, naphtha and absolute ethyl alcohol. The solvent can dilute the high molecular silicon rubber matrix, and creates a favorable environment for the uniform dispersion of the conductive particles and the nano modified particles.
Preferably, a 100-mesh and 300-mesh nylon screen plate is adopted for screen printing in the step (3). The surface of the printed array pressure-sensitive layer is smooth, the thickness is moderate, and a better printing effect can be achieved.
Preferably, the insulating glue is 3M9495LE double-sided glue. The double-sided adhesive is prepared from a transparent PET (polyethylene terephthalate) base material, the adhesive is acrylic adhesive, the double-sided adhesive has good size and thermal stability, moisture resistance and the like, has good viscosity for rubber, plastic and the like, is not easy to wrinkle, is easy to die-cut and process, and provides a basic guarantee for a graphical definition process of a sensor array.
The invention also provides a sandwich type large-area high-density flexible array sensor prepared by the method, which comprises an upper polar plate, a lower polar plate, an array pressure-sensitive layer and an insulating adhesive layer, wherein the array pressure-sensitive layer and the insulating adhesive layer are arranged between the upper polar plate and the lower polar plate, the upper polar plate and the lower polar plate are provided with corresponding array electrodes and leads, one sides of the upper polar plate and the lower polar plate, which are provided with the array electrodes and the leads, are oppositely arranged, the array electrodes are in a row-column structure, each row electrode of one polar plate is connected through the lead, each column electrode of the other polar plate is connected through the lead, and the position of the insulating adhesive layer, which corresponds to the array pressure-sensitive layer, is hollowed.
The sensor with the sandwich structure is prepared by the invention, the sensor consists of the upper polar plate, the lower polar plate and the array pressure sensitive layer positioned between the upper polar plate and the lower polar plate, the array electrodes adopt the array with the row-column structure, the arrangement is uniform, the spatial distribution is reasonable, the manufacturing process is simple, the large-area high-density array is convenient to realize, the position of the insulating adhesive layer corresponding to the pressure sensitive layer of the upper polar plate array and the position of the insulating adhesive layer corresponding to the pressure sensitive layer of the lower polar plate array are hollowed out, so that the upper polar plate and the lower polar plate can be ensured to be contacted with the pressure sensitive layer, and the prepared large-area high-density flexible sensor has high sensitivity and large pressure sensing range.
Preferably, the upper and lower electrode plates are respectively provided with alignment marks corresponding to the four corners of the array electrode. Because the upper electrode and the lower electrode of the sensor with the sandwich structure need to be accurately aligned and packaged, the invention arranges four alignment symbols on the upper polar plate and the lower polar plate, which is beneficial to the accurate alignment of the upper polar plate and the lower polar plate and improves the packaging efficiency.
Therefore, the invention has the following beneficial effects:
(1) the polar plate and the array pressure-sensitive layer are manufactured by adopting a screen printing process, so that the process can be simplified, the cost can be reduced, and the processing efficiency can be improved;
(2) the proportion of each component of the pressure-sensitive composite material is suitable for a screen printing process, the composite material can well penetrate through a screen printing plate during printing, the performance after printing is good, the film thickness is uniform and smooth, and the phenomena of paste surface deformation and the like are avoided;
(3) the pressure-sensitive composite material adopts carbon black and carbon nano tubes as conductive particles together, the carbon black/carbon nano tubes are used in the silicone rubber together to play a role in synergistic enhancement, the carbon black and the carbon nano tubes can form a structure similar to a grape string, silicone rubber molecular chains are used as frameworks of conductive network chains and are mutually staggered with the grape string-shaped structure to form a stable reinforcement structure, and the integral reinforcement structure has certain influence on the conductivity and stability of a composite system and the mechanical property of the composite material;
(4) the alignment marks are arranged on the upper polar plate and the lower polar plate, so that the upper polar plate and the lower polar plate can be accurately aligned, and the packaging efficiency is improved;
(5) pass through the laminating of 3M9495LE double faced adhesive tape with the upper and lower polar plate of sensor, not only can completely cut off silver wire and air contact, also can play the not impaired effect of protection array pressure sensitive layer, and this double faced adhesive tape has good size and thermal stability, and the moisture resistance etc. has fine viscidity to rubber, plastic etc. is difficult for the fold to easily cross cutting processing.
Drawings
FIG. 1 is a schematic view of an exploded structure of a sandwich-type large-area high-density flexible array sensor according to the present invention.
In the figure: 1 upper polar plate, 2 lower polar plate, 3 array pressure sensitive layers, 4 insulating glue layers, 5 array electrodes, 6 leads and 7 alignment marks.
Detailed Description
The invention is further described with reference to the following detailed description and accompanying drawings.
As shown in fig. 1, the sandwich-type large-area high-density flexible array sensor manufactured in each embodiment and comparative example of the present invention includes an upper plate 1, a lower plate 2, an array pressure-sensitive layer 3 and an insulating adhesive layer 4, which are disposed between the upper plate and the lower plate, the insulating adhesive is 3M9495LE double-sided adhesive tape, the upper plate and the lower plate are provided with corresponding array electrodes 5 and leads 6, one side of the upper plate and one side of the lower plate provided with the array electrodes and the leads are disposed oppositely, the array electrodes are arranged in a row 6 × 6 arrangement, the electrodes are circular with a diameter of 0.8cm, the distance between two adjacent electrodes is 1cm, each row of electrodes of the upper plate are connected through the leads, each row of the lower plate is connected through the leads, the position of the insulating adhesive layer corresponding to the array pressure-sensitive layer is hollowed, and four corners of the upper plate and the lower plate corresponding to the array electrodes are respectively provided with cross-shaped alignment marks 7.
According to the invention, before preparing the polar plate, a PET substrate with the thickness of 0.125mm is cut into the size of 8cm multiplied by 8cm according to the size occupied by the required electrode and the wire, the cut PET substrate is cleaned by absolute ethyl alcohol and deionized water, surface impurities are removed, the adhesive force of a printing material is improved, and then a silk screen plate is manufactured according to the electrode and wire patterns.
Example 1:
preparing a polar plate: respectively printing Yttnew ID01 type conductive silver paste on two PET substrates by using a 420-mesh steel wire mesh plate through a screen printing process, forming array electrodes and leads which correspond to each other on the two PET substrates, placing the printed PET substrates in a forced air oven, and drying the PET substrates at 120 ℃ for 40min to obtain upper and lower polar plates;
preparing a pressure-sensitive composite material: 20g of Keqin carbon black ECP600JD, 5g of carbon nano tube and 5g of nano SiO2Adding 10g of 2% silane coupling agent Si-69 into 85g of naphtha, stirring, performing ultrasonic dispersion for 30min to form dispersion liquid, adding 350g of room temperature vulcanized silicone rubber Dow Corning 184 into the dispersion liquid, performing magnetic stirring for 3h at room temperature to form viscous mixed liquid, placing the mixed liquid into a vacuum drying oven, drying for 20min at 40 ℃, and removing bubbles and incompletely volatilized naphtha to obtain the uncured pressure-sensitive composite material;
manufacturing a pressure-sensitive layer of the sensor array: the method comprises the following steps of printing an uncured pressure-sensitive composite material on an array electrode on a lower polar plate by using a 300-mesh nylon screen plate through a screen printing process to form an array pressure-sensitive layer, and performing printing once again after the composite material layer is completely cured in one-time printing in order to avoid the problems of cracks and the like of the composite material layer possibly existing to the greatest extent, so that the effectiveness of a sensor is ensured;
packaging a sensor: and aligning the array electrodes on the upper polar plate and the lower polar plate with the cross-shaped alignment mark, and attaching the two-sided adhesive tape through 3M9495LE to obtain the sandwich-type large-area high-density flexible array sensor.
Example 2:
preparing a polar plate: respectively printing Ust new ID01 type conductive silver paste on two PET substrates by using a 300-mesh polyester screen plate through a screen printing process, forming array electrodes and leads which correspond to each other on the two PET substrates, placing the printed PET substrates in a forced air oven, and drying the PET substrates at 140 ℃ for 60min to obtain upper and lower polar plates;
preparing a pressure-sensitive composite material: 75g of Keqin carbon black ECP600JD, 25g of carbon nano tube and 20g of nano SiO2And 40g of 2% silane coupling agent Si-69, 25g of n-hexane, 65g of naphtha and 25g of absolute ethyl alcohol were added to the mixture to mixMixing the solution, stirring, performing ultrasonic dispersion for 60min to form a dispersion solution, adding 450g of room-temperature vulcanized silicone rubber downing 184 into the dispersion solution, performing magnetic stirring for 8h at room temperature to form a viscous mixed solution, placing the mixed solution in a vacuum drying oven, drying for 30min at 100 ℃, and removing bubbles and solvent which is not completely volatilized to obtain the uncured pressure-sensitive composite material;
manufacturing a pressure-sensitive layer of the sensor array: printing an uncured pressure-sensitive composite material on an array electrode on a lower polar plate by using a 100-mesh nylon screen plate through a screen printing process to form an array pressure-sensitive layer, and performing printing once again after the printing is completely cured to ensure the effectiveness of the sensor in order to avoid the possible problems of cracks and the like of the composite material layer as much as possible;
packaging a sensor: and aligning the array electrodes on the upper polar plate and the lower polar plate with the cross-shaped alignment mark, and attaching the two-sided adhesive tape through 3M9495LE to obtain the sandwich-type large-area high-density flexible array sensor.
Example 3:
preparing a polar plate: respectively printing Yttnew ID01 type conductive silver paste on two PET substrates by using a 400-mesh polyester screen plate through a screen printing process, forming array electrodes and leads which correspond to each other on the two PET substrates, placing the printed PET substrates in a forced air oven, and drying the PET substrates at 130 ℃ for 50min to obtain upper and lower polar plates;
preparing a pressure-sensitive composite material: 50g of Keqin carbon black ECP600JD, 10g of carbon nano tube and 15g of nano SiO2Adding 30g of 2% silane coupling agent Si-69 into a mixed solution of 70g of naphtha and 30g of absolute ethyl alcohol, stirring and then ultrasonically dispersing for 40min to form a dispersion liquid, adding 400g of room-temperature vulcanized silicone rubber Dow Corning 184 into the dispersion liquid, magnetically stirring for 6h at room temperature to form a viscous mixed liquid, placing the mixed liquid into a vacuum drying oven to dry for 25min at 70 ℃, and removing bubbles, naphtha which is not completely volatilized and absolute ethyl alcohol to obtain an uncured pressure-sensitive composite material;
manufacturing a pressure-sensitive layer of the sensor array: the method comprises the following steps of printing an uncured pressure-sensitive composite material on an array electrode on a lower polar plate by using a 200-mesh nylon screen plate through a screen printing process to form an array pressure-sensitive layer, and performing printing once again after the composite material layer is completely cured in one-time printing to avoid the possible problems of cracks and the like of the composite material layer to the greatest extent so as to ensure the effectiveness of a sensor;
packaging a sensor: and aligning the array electrodes on the upper polar plate and the lower polar plate with the cross-shaped alignment mark, and attaching the two-sided adhesive tape through 3M9495LE to obtain the sandwich-type large-area high-density flexible array sensor.
Example 4:
preparing a polar plate: respectively printing Yttnew ID01 type conductive silver paste on two PET substrates by using a 420-mesh steel wire mesh plate through a screen printing process, forming array electrodes and leads which correspond to each other on the two PET substrates, placing the printed PET substrates in a forced air oven, and drying the PET substrates at 120 ℃ for 40min to obtain upper and lower polar plates;
preparing surface modified conductive particles: dispersing 20g of Keqin carbon black ECP600JD and 5g of carbon nano tubes in 0.4mol/L nitric acid solution, carrying out oscillation reaction for 3h, filtering, washing with water to be neutral, and drying at 70 ℃ for 24 h; the resulting product was dissolved in SOCl2Dropwise adding two drops of N, N-dimethylformamide, and reacting at 60 ℃ for 24 hours; dispersing the obtained product in ethylene glycol, and carrying out reflux reaction for 30h at the temperature of 120 ℃; to the resulting product were added 1.67g 4-dimethylaminopyridine, 16.7g triethylamine and 532mL CHCl3Mixing, adding a solution of 25g of 2-bromoisobutyl acyl bromide dissolved in 250mL of chloroform under the protection of nitrogen, stirring at 4 ℃ for 2h, and continuing to react at room temperature for 30 h; diluting the obtained solution with chloroform, filtering, repeatedly washing, and drying at 60 deg.C for 20 h; mixing the dried product with 5g of pentamethyldiethylenetriamine, 5g of CuBr and 250mL of N, N-dimethylformamide, adding 250g of vinyl pyrrolidone under the protection of nitrogen, and stirring and reacting at 70 ℃ for 30 hours; after the obtained solution is filtered, washing the solution to be neutral by water, and drying the solution for 12 hours at 70 ℃ to obtain surface modified conductive particles;
preparing a pressure-sensitive composite material: 25g of the surface-modified conductive particles prepared above and 5g of nano SiO2And 10g of 2% silane coupling agent Si-69, added into 85g of naphtha, stirred and ultrasonically dispersed for 30min to form a dispersion liquid. Adding 350g of room temperature vulcanized silicone rubber Dow Corning 184 into the dispersion, magnetically stirring for 3h at room temperature to form a viscous mixture, and placing the viscous mixture in a vacuumDrying in an air drying oven at 40 deg.C for 20min to remove air bubbles and incompletely volatilized naphtha to obtain uncured pressure-sensitive composite material; manufacturing a pressure-sensitive layer of the sensor array: the method comprises the following steps of printing an uncured pressure-sensitive composite material on an array electrode on a lower polar plate by using a 300-mesh nylon screen plate through a screen printing process to form an array pressure-sensitive layer, and performing printing once again after the composite material layer is completely cured in one-time printing in order to avoid the problems of cracks and the like of the composite material layer possibly existing to the greatest extent, so that the effectiveness of a sensor is ensured;
packaging a sensor: and aligning the array electrodes on the upper polar plate and the lower polar plate with the cross-shaped alignment mark, and attaching the two-sided adhesive tape through 3M9495LE to obtain the sandwich-type large-area high-density flexible array sensor.
Example 5:
preparing a polar plate: respectively printing Ust new ID01 type conductive silver paste on two PET substrates by using a 300-mesh polyester screen plate through a screen printing process, forming array electrodes and leads which correspond to each other on the two PET substrates, placing the printed PET substrates in a forced air oven, and drying the PET substrates at 140 ℃ for 60min to obtain upper and lower polar plates;
preparing surface modified conductive particles: dispersing 75g of Keqin carbon black ECP600JD and 25g of carbon nano tubes in 0.5mol/L nitric acid solution, carrying out oscillation reaction for 2.5h, filtering, washing with water to be neutral, and drying at 65 ℃ for 20 h; the resulting product was dissolved in SOCl2Dropwise adding 3 drops of N, N-dimethylformamide, and reacting at 55 ℃ for 20 hours; dispersing the obtained product in ethylene glycol, and carrying out reflux reaction for 25h at the temperature of 110 ℃; to the resulting product were added 5g of 4-dimethylaminopyridine, 75g of triethylamine and 2150mL of CHCl3Mixing, adding a solution of 2-bromoisobutyl acyl bromide dissolved in 2000mL chloroform under the protection of nitrogen, stirring at 2 ℃ for 1.5h, and continuing to react at room temperature for 25 h; diluting the obtained solution with chloroform, filtering, repeatedly washing, and drying at 55 deg.C for 15 h; mixing the dried product with 14.3g of pentamethyldiethylenetriamine, 28.6g of CuBr and 1000mL of N, N-dimethylformamide, adding 1500g of vinyl pyrrolidone under the protection of nitrogen, and stirring and reacting at 65 ℃ for 25 h; after the obtained solution is filtered, washing the solution to be neutral by water, and drying the solution for 8 hours at 65 ℃ to obtain surface modified conductive particles;
preparation ofPressure sensitive composite material: 100g of the surface-modified conductive particles prepared above and 20g of nano SiO2Adding 40g of 2% silane coupling agent Si-69 into a mixed solution of 25g of n-hexane, 65g of naphtha and 25g of absolute ethyl alcohol, stirring and then ultrasonically dispersing for 60min to form a dispersion liquid, adding 450g of room temperature vulcanized silicone rubber Dow Corning 184 into the dispersion liquid, magnetically stirring for 8h at room temperature to form a viscous mixed liquid, placing the mixed liquid into a vacuum drying oven to dry for 30min at 100 ℃, and removing bubbles and incompletely volatilized solvent to obtain the uncured pressure-sensitive composite material;
manufacturing a pressure-sensitive layer of the sensor array: printing an uncured pressure-sensitive composite material on an array electrode on a lower polar plate by using a 100-mesh nylon screen plate through a screen printing process to form an array pressure-sensitive layer, and performing printing once again after the printing is completely cured to ensure the effectiveness of the sensor in order to avoid the possible problems of cracks and the like of the composite material layer as much as possible;
packaging a sensor: and aligning the array electrodes on the upper polar plate and the lower polar plate with the cross-shaped alignment mark, and attaching the two-sided adhesive tape through 3M9495LE to obtain the sandwich-type large-area high-density flexible array sensor.
Example 6:
preparing a polar plate: respectively printing Yttnew ID01 type conductive silver paste on two PET substrates by using a 400-mesh polyester screen plate through a screen printing process, forming array electrodes and leads which correspond to each other on the two PET substrates, placing the printed PET substrates in a forced air oven, and drying the PET substrates at 130 ℃ for 50min to obtain upper and lower polar plates;
preparing surface modified conductive particles: dispersing 50g of Keqin carbon black ECP600JD and 10g of carbon nano tubes in 0.6mol/L nitric acid solution, carrying out oscillation reaction for 2h, filtering, washing with water to be neutral, and drying at 60 ℃ for 12 h; the resulting product was dissolved in SOCl2Dropwise adding two drops of N, N-dimethylformamide, and reacting at 50 ℃ for 12 hours; dispersing the obtained product in ethylene glycol, and carrying out reflux reaction for 20h at 100 ℃; to the resulting product was added 3.3g 4-dimethylaminopyridine, 40g triethylamine and 1200mL CHCl3Mixing, adding a solution of 90g of 2-bromoisobutylacyl bromide in 650mL of chloroform under nitrogen, stirring at 0 deg.C for 1h, and continuing at room temperatureReacting for 20 hours; diluting the obtained solution with chloroform, filtering, repeatedly washing, and drying at 50 deg.C for 10 hr; mixing the dried product with 10g of pentamethyldiethylenetriamine, 15g of CuBr and 600mL of N, N-dimethylformamide, adding 720g of vinyl pyrrolidone under the protection of nitrogen, and stirring and reacting for 20 hours at 60 ℃; after the obtained solution is filtered, washing the solution to be neutral by water, and drying the solution for 6 hours at the temperature of 60 ℃ to obtain surface modified conductive particles;
preparing a pressure-sensitive composite material: 60g of the surface-modified conductive particles prepared above and 15g of nano SiO2And 30g of 2% silane coupling agent Si-69, adding into a mixed solution of 70g of naphtha and 30g of absolute ethyl alcohol, stirring, and performing ultrasonic dispersion for 40min to form a dispersion liquid. Adding 400g of room-temperature vulcanized silicone rubber downing 184 into the dispersion, magnetically stirring for 6 hours at room temperature to form viscous mixed liquid, placing the mixed liquid in a vacuum drying oven, drying for 25 minutes at 70 ℃, and removing bubbles, naphtha which is not completely volatilized and absolute ethyl alcohol to obtain an uncured pressure-sensitive composite material;
manufacturing a pressure-sensitive layer of the sensor array: printing an uncured pressure-sensitive composite material on the array electrode on the lower polar plate by using a 200-mesh nylon screen plate through a screen printing process to form an array pressure-sensitive layer;
packaging a sensor: and aligning the array electrodes on the upper polar plate and the lower polar plate with the cross-shaped alignment mark, and attaching the two-sided adhesive tape through 3M9495LE to obtain the sandwich-type large-area high-density flexible array sensor.
Comparative example 1:
preparing a polar plate: respectively printing Yttnew ID01 type conductive silver paste on two PET substrates by using a 420-mesh steel wire mesh plate through a screen printing process, forming array electrodes and leads which correspond to each other on the two PET substrates, placing the printed PET substrates in a forced air oven, and drying the PET substrates at 120 ℃ for 40min to obtain upper and lower polar plates;
preparing a pressure-sensitive composite material: 25g of Keqin carbon black ECP600JD and 20g of nano SiO2And 40g of 2% silane coupling agent Si-69, added into 115g of naphtha, stirred and ultrasonically dispersed for 30min to form a dispersion liquid. Adding 450g of room temperature vulcanized silicone rubber into the dispersion, magnetically stirring for 3 hours at room temperature to form a viscous mixed solution, and placing the mixed solution in a containerDrying in a vacuum drying oven at 40 ℃ for 20min to remove air bubbles and incompletely volatilized naphtha to obtain an uncured pressure-sensitive composite material;
manufacturing a pressure-sensitive layer of the sensor array: the method comprises the following steps of printing an uncured pressure-sensitive composite material on an array electrode on a lower polar plate by using a 300-mesh nylon screen plate through a screen printing process to form an array pressure-sensitive layer, and performing printing once again after the composite material layer is completely cured in one-time printing in order to avoid the problems of cracks and the like of the composite material layer possibly existing to the greatest extent, so that the effectiveness of a sensor is ensured;
packaging a sensor: and aligning the array electrodes on the upper polar plate and the lower polar plate with the cross-shaped alignment mark, and attaching the two-sided adhesive tape through 3M9495LE to obtain the sandwich-type large-area high-density flexible array sensor.
The performance test of the sandwich-type large-area high-density flexible array sensor prepared in the above examples and comparative examples is performed, and the test results are shown in table 1.
Table 1: and (5) testing the performance of the sandwich type large-area high-density flexible array sensor.
As can be seen from Table 1, the sensor has a significant negative pressure resistance effect only in the range of 0-4N when only carbon black is used as the conductive particle in comparative example 1, while the sensor has a significant negative pressure resistance effect in the range of 0-7N and above when carbon black and carbon nanotubes are used together as the conductive particle in examples 1-6, so that the pressure sensing range of the sensor is wider when carbon black and carbon nanotubes are used together as the conductive particle.
The sensitivity of the sensor is 2k omega/N or less when the ordinary conductive particles are used in the embodiments 1-3, and the sensitivity of the sensor can be increased to 2.9-3.1k omega/N when the surface modified conductive particles are used in the embodiments 4-6, so that the sensor can have higher sensitivity when the surface modified conductive particles are used.
Claims (9)
1. A preparation method of a sandwich type large-area high-density flexible array sensor is characterized by comprising the following steps:
(1) preparing a polar plate: respectively printing electrode materials on the two substrate materials by adopting a screen printing process, forming an array electrode and a lead which correspond to each other on the two substrate materials, and drying to obtain an upper polar plate and a lower polar plate;
(2) preparing a pressure-sensitive composite material: the conductive particles and 5-20 parts of nano SiO by weight2And 15-40 parts of silane coupling agent Si-69 are dispersed in 85-115 parts of solvent to form dispersion liquid; adding 350-450 parts of silicon rubber into the dispersion liquid, and uniformly stirring to obtain a mixed liquid; vacuum drying the mixed solution for 20-30min to obtain an uncured pressure-sensitive composite material, wherein the conductive particles comprise 20-75 parts of carbon black and 5-25 parts of carbon nanotubes;
the conductive particles are surface-modified conductive particles, and the preparation method comprises the following steps:
(A) dispersing conductive particles in 0.4-0.6mol/L nitric acid solution, carrying out oscillation reaction for 2-3h, filtering, washing with water to neutrality, and drying at 60-70 ℃ for 12-24 h;
(B) dissolving the obtained product in thionyl chloride, adding 2-3 drops of N, N-dimethylformamide, and reacting at 50-60 ℃ for 12-24 h;
(C) dispersing the obtained product in ethylene glycol, and carrying out reflux reaction at the temperature of 100-120 ℃ for 20-30 h;
(D) mixing 4-dimethylamino pyridine and triethylamine in the mass ratio of 1 (10-15) to (15-20) and the product obtained in the step (C), adding CHCl3Adding a chloroform solution of 2-bromoisobutyl acyl bromide with the mass ratio of 1:1-2:1 to the product obtained in the step (C) under the protection of nitrogen, stirring at 0-4 ℃ for 1-2h, and continuing to react at room temperature for 20-30 h;
(E) diluting the obtained solution with chloroform, filtering, repeatedly washing, and drying at 50-60 deg.C for 10-20 h;
(F) mixing the dried pentamethyl diethylenetriamine and CuBr in the mass ratio of 1 (1-2) to 5-7 with the product obtained in the step (E), adding N, N-dimethylformamide, adding vinyl pyrrolidone in the mass ratio of 10:1-15:1 with the product obtained in the step (E) under the protection of nitrogen, and stirring and reacting for 20-30h at the temperature of 60-70 ℃;
(G) after the obtained solution is filtered, washing the solution to be neutral by water, and drying the solution for 6 to 12 hours at the temperature of between 60 and 70 ℃ to obtain surface modified conductive particles;
(3) manufacturing a pressure-sensitive layer of the sensor array: printing an uncured pressure-sensitive composite material on the array electrode on one of the polar plates by adopting a screen printing process, and forming an array pressure-sensitive layer after curing;
(4) packaging a sensor: and (4) attaching the upper and lower polar plates through insulating glue.
2. The method as claimed in claim 1, wherein the electrode material in step (1) is Eudragit ID01 conductive silver paste, and the base material is PET substrate.
3. The method for preparing a sandwich-type large-area high-density flexible array sensor according to claim 1 or 2, wherein a 300-420 mesh steel wire mesh plate or a polyester mesh plate is used for screen printing in the step (1).
4. The method for preparing a sandwich-type large-area high-density flexible array sensor according to claim 1 or 2, wherein the drying temperature in step (1) is 120 ℃ and 140 ℃, and the drying time is 40-60 min.
5. The method for preparing a sandwich-type large-area high-density flexible array sensor according to claim 1 or 4, wherein the solvent in the step (2) comprises at least one of n-hexane, naphtha and absolute ethyl alcohol.
6. The method as claimed in claim 1, wherein a 100-mesh and 300-mesh nylon screen is used for screen printing in step (3).
7. The method for preparing a sandwich-type large-area high-density flexible array sensor according to claim 1, wherein the insulating adhesive is 3M9495LE double-sided adhesive.
8. A sandwich type large-area high-density flexible array sensor prepared according to the method of claim 1 is characterized by comprising an upper polar plate, a lower polar plate, an array pressure-sensitive layer and an insulating adhesive layer, wherein the array pressure-sensitive layer and the insulating adhesive layer are arranged between the upper polar plate and the lower polar plate, corresponding array electrodes and corresponding leads are arranged on the upper polar plate and the lower polar plate, one sides of the upper polar plate and the lower polar plate, which are provided with the array electrodes and the corresponding leads, are oppositely arranged, the array electrodes are in a row-column structure, each row electrode of one polar plate is connected through the corresponding lead, each column electrode of the other polar plate is connected through the corresponding lead, and the position of the insulating adhesive layer, which corresponds to the array pressure-sensitive layer, is hollowed.
9. The sandwich-type large-area high-density flexible array sensor as claimed in claim 8, wherein alignment marks are respectively provided at four corners of the upper and lower electrode plates corresponding to the array electrodes.
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